CN106009537A - Full-biodegrade composite material taking oriented poly butylene succinate as nucleating agent and preparation method of full-biodegrade composite material - Google Patents
Full-biodegrade composite material taking oriented poly butylene succinate as nucleating agent and preparation method of full-biodegrade composite material Download PDFInfo
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- CN106009537A CN106009537A CN201610355020.XA CN201610355020A CN106009537A CN 106009537 A CN106009537 A CN 106009537A CN 201610355020 A CN201610355020 A CN 201610355020A CN 106009537 A CN106009537 A CN 106009537A
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- butylene succinate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention provides a full-biodegrade composite material taking oriented poly butylene succinate as a nucleating agent and a preparation method of the full-biodegrade composite material. The full-biodegrade composite material comprises the following components in mass percent: 30-70% of poly butylene succinate and 70-30% of poly ethylene succinate. The preparation method comprises the following steps: 1) drying poly ethylene succinate in vacuum at 25-40 DEG C, and drying poly butylene succinate in vacuum at 60-100 DEG C; 2) putting 0-100% of poly ethylene succinate and 0-100% of poly butylene succinate into a screw extruder, and carrying out blending and extruding to obtain a composite material; 3) carrying out single-side rolling and plate pressing on the composite material of poly ethylene succinate and poly butylene succinate at appropriate processing temperature; and 4) taking out the molded composite material, and carrying out heat treatment on the molded composite material at the temperature below the melting point of poly ethylene succinate, so as to obtain the composite material. The full-biodegrade composite material is simple and feasible in process, low in cost, easy to realize industrialization and obvious in economic value.
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to be orientated poly butylene succinate as nucleation
Biodegradable composite material of agent and preparation method thereof.
Background technology
The advantages such as poly-succinic fourth diester (PBS) as aliphatic polyester has heat stability height, high molecular, but its
Symmetry is high, and degree of crystallinity is high, makes its biodegradation rate be affected, and its toughness, elongation at break, intensity etc. are square
Face all existing defects.As a kind of polymorphous aliphatic poly ester material, polyadipate fourth diester (PBA) has the biology of excellence
Degradation property, has a wide range of applications in fields such as packaging for foodstuff, agricultural mulching, biological medicines.Can be as environmentally friendly
Degradable material is applied.Its fusing point is relatively low, and degradation rate is good.By making PBA Yu PBS composite, it is possible not only to improve PBS
Toughness, elongation at break, the defect of the aspect such as intensity, and we can realize full aliphatic by regulation and control PBA crystal formation and be combined
The controllability of material degradation speed.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide to be orientated poly butylene succinate as nucleation
Biodegradable composite material of agent and preparation method thereof, can obtain crystallizing fast, intensity height by the method, and degradation rate is good,
Heat stability is high, and the poly adipate succinic acid ester of good toughness and poly butylene succinate composite, the present invention has technique
Feature simply, easy to operation, that cheaper starting materials is easy to get.
To achieve these goals, the technical solution used in the present invention is: to be orientated poly butylene succinate as nucleation
The biodegradable composite material of agent, by mass percentage, including following components:
Poly butylene succinate 30～70%, poly adipate succinic acid ester 70～30%.
Described poly butylene succinate is orientated during Polymer Processing.
The molecular weight of described poly butylene succinate is 10000, and the molecular weight of poly adipate succinic acid ester is 12000.
With the preparation method being orientated the poly butylene succinate biodegradable composite material as nucleator, including following
Step:
1) poly adipate succinic acid ester is dried 3～8 hours under 25～40 DEG C of vacuum, poly butylene succinate 60～
It is dried 3～8 hours under 100 DEG C of vacuum；
2) by 30～the poly adipate succinic acid ester of 70% and 70～the poly butylene succinate mechanical blending of 30%, will be after mixing
Powder put in screw extruder be blended and extrude obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3) poly adipate succinic acid ester is placed an order the processing temperature of 113～118 DEG C with poly butylene succinate composite
Face roller is dynamic, plate pressure, and the pressure of described composite is 150～600MPa, by the time of single constant pressure be 150～
200s；
4) composite after molding is taken out, below the fusing point of poly adipate succinic acid ester, it is carried out heat treatment.
Composite puller system is tested its hot strength；Differential scanning calorimeter is used to test its thermodynamic stability
And crystallization rate；Use the morphosis of its interface zone of polarized light microscope observing, use its configuration of surface of scanning electron microscopic observation.
The invention has the beneficial effects as follows:
Poly-succinic fourth diester, is the thermoplastic of monoclinic system white crystalline, and it, with biological succinic acid as raw material, is compared
In traditional plastic materials, it does not relies on limited petroleum resources, and PBS Heat stability is good, molecular weight are high, symmetry
High, degree of crystallinity is excellent, processability is excellent, biodegradation rate is good.Polyadipate fourth diester (PBA) has excellent flexibility
And crystal property, and degradation property is prominent.Have a wide range of applications in fields such as packaging for foodstuff, agricultural mulching, biological medicines.Its
The more stable α phase crystal of thermodynamics has higher degradation rate compared to β phase crystal, can be as environmentally friendly degraded
Materials application.
Orientation poly butylene succinate, in addition to having good chemical resistance, heat-resisting quantity, also has crystallization
More complete, the advantages such as crystallization is quick, with short production cycle.Using orientation poly butylene succinate as nucleator, it is possible not only to
Improve the crystalline rate of poly adipate succinic acid ester, shorten its production cycle, due to poly butylene succinate and polyadipate
Oxygen in butanediol ester strand can be with the hydrogen evolution hydrogen bond of the end of the chain, it is also possible to the effective composite material interface that improves combines strong
Degree, gives complete biodegradable system composite with excellent mechanical property and thermal stability.
Accompanying drawing explanation
Fig. 1 is the poly adipate succinic acid ester composite crystalline rate design sketch of the present invention, and wherein Fig. 1 (a) is for implementing
The design sketch of example one；Fig. 1 (b) is the design sketch of embodiment two.
Fig. 2 is the design sketch of the crystallization temperature of the poly adipate succinic acid ester composite of the present invention, and wherein Fig. 2 (a) is
The design sketch of embodiment one；Fig. 2 (b) is the design sketch of embodiment three.
Fig. 3 is the design sketch of the poly adipate succinic acid ester composite of embodiments of the invention one, embodiment four.
Detailed description of the invention
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment one
The preparation method of the poly adipate succinic acid ester composite with poly butylene succinate as nucleator, its feature exists
In, comprise the following steps:
1) being dried 3 hours under 40 DEG C of vacuum by poly adipate succinic acid ester, poly butylene succinate is dry under 100 DEG C of vacuum
Dry 3 hours；
2) by 30% poly adipate succinic acid ester and the poly butylene succinate mechanical blending of 70%, mixed powder is put
Entering to be blended in screw extruder and extrude and obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3) to poly adipate succinic acid ester and poly butylene succinate composite one side roller under the processing temperature of 115 DEG C
Dynamic, plate pressure；The pressure of described composite is 150Pa, is 150s by the time of single constant pressure；
4) composite after molding is taken out, at 40 DEG C, it is carried out heat treatment.
Composite puller system is tested its hot strength；Use the form knot of its interface zone of polarized light microscope observing
Structure, uses differential scanning calorimeter to test its thermodynamic stability and crystallization temperature；Use its interface of scanning electron microscopic observation and cut
Face form.Use wide-angle X ray diffractor that it is carried out the mensuration of crystal formation.The hot strength of poly adipate succinic acid ester thin film is
40.1MPa, poly adipate succinic acid ester crystallization peak temperature is 31.05 DEG C.
Embodiment two
With the preparation method being orientated the poly butylene succinate biodegradable composite material as nucleator, it is characterised in that
Comprise the following steps:
1) being dried 8 hours under 25 DEG C of vacuum by poly adipate succinic acid ester, orientation poly butylene succinate is in 60 DEG C of vacuum
Under be dried 8 hours；
2) by 50% poly adipate succinic acid ester and the poly butylene succinate mechanical blending of 50%, mixed powder is put
Entering to be blended in screw extruder and extrude and obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3) poly adipate succinic acid ester and poly butylene succinate composite are carried out one side roller the processing temperature of 116 DEG C
Dynamic, plate pressure；The pressure of described composite is 400Pa, is 170s by the time of single constant pressure；
4) composite after molding is taken out, at 30 DEG C, it is carried out heat treatment.
Composite puller system is tested its hot strength；Differential scanning calorimeter is used to test its thermodynamic stability
And crystallization rate；Use the morphosis of its interface zone of polarized light microscope observing, use its configuration of surface of scanning electron microscopic observation.
Use wide-angle X ray diffractor that it is carried out the mensuration of crystal formation.The hot strength of poly adipate succinic acid ester composite is
38.7 MPa, poly adipate succinic acid ester crystallization peak temperature is 37.4 DEG C.
Embodiment three
With the preparation method being orientated the poly butylene succinate biodegradable composite material as nucleator, it is characterised in that
Comprise the following steps:
1) being dried 8 hours under 25 DEG C of vacuum by poly adipate succinic acid ester, orientation poly butylene succinate is in 60 DEG C of vacuum
Under be dried 8 hours；
2) by 70% poly adipate succinic acid ester and the poly butylene succinate mechanical blending of 30%, mixed powder is put
Entering to be blended in screw extruder and extrude and obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3), plate pressure dynamic with poly butylene succinate composite one side roller at 118 DEG C to poly adipate succinic acid ester；Described
The pressure of composite is 600Pa, is 200s by the time of single constant pressure；
4) composite after molding is taken out, at 0 DEG C, it is carried out heat treatment.
Composite puller system is tested its hot strength；Differential scanning calorimeter is used to test its thermodynamic stability
And crystallization rate；Use the morphosis of its interface zone of polarized light microscope observing, use its configuration of surface of scanning electron microscopic observation.
Use wide-angle X ray diffractor that it is carried out the mensuration of crystal formation.Then the hot strength of poly adipate succinic acid ester composite is
35.5MPa, poly adipate succinic acid ester crystallization peak temperature is 38.6 DEG C.
Seeing the polarisation figure that Fig. 1, Fig. 1 upper right corner is pure poly adipate succinic acid ester (PBA) material, the lower left corner is for implementing
The polarisation figure of poly adipate succinic acid ester (PBA) composite of example 1；As it can be seen, it is multiple with poly butylene succinate (PBS)
In the material closed, poly adipate succinic acid ester (PBA) is without spherocrystal pattern, and pure own without poly butylene succinate (PBS) component
Succinate adipate (PBA) is then grown to pattern spherulitic crystal structure clearly.
See the microstructure figure of poly adipate succinic acid ester (PBA) composite that Fig. 2, Fig. 2 are embodiment 2, in figure
Direction shown in arrow is the direction that poly butylene succinate (PBS) shears orientation, as it can be seen, tetramethylene adipate
(PBA) direction being perpendicular to poly butylene succinate (PBS) is grown to serve as orderly crystal structure.
See the crystalline rate figure that Fig. 3, Fig. 3 are embodiment 3.Abscissa is crystallization temperature, and vertical coordinate is enthalpy.As schemed
Showing, after compound with poly butylene succinate (PBS) shearing, the crystallization temperature of tetramethylene adipate (PBA) is significantly raised,
Crystallization in advance, illustrates that the poly butylene succinate (PBS) of orientation has excellent nucleation to it,.
Hot strength testing standard: GB/T 1040.1-2006
Crystallization temperature test condition: material is lowered the temperature with 5 DEG C/min by molten state
From above-described embodiment it can be seen that with the PBS crystallization rate of composite of PBA as nucleator of orientation, mechanical property
The energy PBA relative with pure with thermodynamic stability is obtained for and is greatly improved, and learns through wide-angle x-ray detection, multiple
In condensation material, the crystal formation of PBA is not influenced by temperature, and is all its degradation rate faster α phase crystal in embodiment 1,2 and 3,
Therefore, its crystalline rate, hot strength and thermodynamic stability, on the basis of improve PBA degradation rate, are had by the present invention
Significantly promote, have important meaning for environmental conservation, and improve crystallization temperature, accelerate its process-cycle, no
Only having eco-friendly advantage, and have great economic benefit, market potential is huge.
Claims (7)
1. to be orientated the poly butylene succinate biodegradable composite material as nucleator, it is characterised in that by quality hundred
Proportion by subtraction, including following components:
Poly butylene succinate 30～70%, poly adipate succinic acid ester 70～30%.
It is the most according to claim 1 to be orientated the poly butylene succinate biodegradable composite material as nucleator,
It is characterized in that, described poly butylene succinate is orientated during Polymer Processing.
It is the most according to claim 2 to be orientated the poly butylene succinate biodegradable composite material as nucleator,
It is characterized in that, the molecular weight of described poly butylene succinate is 10000, and the molecular weight of poly adipate succinic acid ester is
12000。
4., with the preparation method being orientated the poly butylene succinate biodegradable composite material as nucleator, its feature exists
In, comprise the following steps:
1) poly adipate succinic acid ester is dried 3～8 hours under 25～40 DEG C of vacuum, poly butylene succinate 60～
It is dried 3～8 hours under 100 DEG C of vacuum；
2) by 30～the poly adipate succinic acid ester of 70% and 70～the poly butylene succinate mechanical blending of 30%, will be after mixing
Powder put in screw extruder be blended and extrude obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3) poly adipate succinic acid ester is placed an order the processing temperature of 113～118 DEG C with poly butylene succinate composite
Face roller is dynamic, plate pressure, and the pressure of described composite is 150～600MPa, by the time of single constant pressure be 150～
200s；
4) composite after molding is taken out, below the fusing point of poly adipate succinic acid ester, it is carried out heat treatment.
Poly adipate succinic acid ester composite with poly butylene succinate as nucleator the most according to claim 4
Preparation method, it is characterised in that comprise the following steps:
1) being dried 3 hours under 40 DEG C of vacuum by poly adipate succinic acid ester, poly butylene succinate is dry under 100 DEG C of vacuum
Dry 3 hours；
2) by 30% poly adipate succinic acid ester and the poly butylene succinate mechanical blending of 70%, mixed powder is put
Entering to be blended in screw extruder and extrude and obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3) to poly adipate succinic acid ester and poly butylene succinate composite one side roller under the processing temperature of 115 DEG C
Dynamic, plate pressure；The pressure of described composite is 150Pa, is 150s by the time of single constant pressure；
4) composite after molding is taken out, at 40 DEG C, it is carried out heat treatment.
The most according to claim 4 with the orientation poly butylene succinate biodegradable composite material as nucleator
Preparation method, it is characterised in that comprise the following steps:
1) being dried 8 hours under 25 DEG C of vacuum by poly adipate succinic acid ester, orientation poly butylene succinate is in 60 DEG C of vacuum
Under be dried 8 hours；
2) by 50% poly adipate succinic acid ester and the poly butylene succinate mechanical blending of 50%, mixed powder is put
Entering to be blended in screw extruder and extrude and obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3) poly adipate succinic acid ester and poly butylene succinate composite are carried out one side roller the processing temperature of 116 DEG C
Dynamic, plate pressure；The pressure of described composite is 400Pa, is 170s by the time of single constant pressure；
4) composite after molding is taken out, at 30 DEG C, it is carried out heat treatment.
The most according to claim 5 with the orientation poly butylene succinate biodegradable composite material as nucleator
Preparation method, it is characterised in that comprise the following steps:
1) being dried 8 hours under 25 DEG C of vacuum by poly adipate succinic acid ester, orientation poly butylene succinate is in 60 DEG C of vacuum
Under be dried 8 hours；
2) by 70% poly adipate succinic acid ester and the poly butylene succinate mechanical blending of 30%, mixed powder is put
Entering to be blended in screw extruder and extrude and obtain composite, the temperature of described screw extruder is 90～200 DEG C；
3), plate pressure dynamic with poly butylene succinate composite one side roller at 118 DEG C to poly adipate succinic acid ester；Described
The pressure of composite is 600Pa, is 200s by the time of single constant pressure；
4) composite after molding is taken out, at 0 DEG C, it is carried out heat treatment.
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| CN201610355020.XA CN106009537A (en) | 2016-05-26 | 2016-05-26 | Full-biodegrade composite material taking oriented poly butylene succinate as nucleating agent and preparation method of full-biodegrade composite material |
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